Process of making aluminum fluorid and other aluminum compounds.



P. A. EMANUEL. PROCESS OF MAKING ALUMINUM FLUORID AND OTHER ALUMINUMCOMPOUNDS.

APPLICATION IILE D MAY 29, 1909.

Patel lted May 10, 1910.

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v I U P ABMANUEL. PROGESS OF MAKING ALUMINUM FLUOBID AND OTHER ALUMINUMCOMPOUNDS.

APPLIG'ATION IILEID MAY 29, N09. 957,754. Patented May 10,1910

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4 PHILIP A. EQFANUEC I 'AIKEN, SOUTH CAROLINA.

PROCESS OF MAKING ,FLUORID AND OTfiEfiALUMINUM COMPOUNDS.

exact descr'i will enable it apperteiu s'lto (My invention "makingelumin miuu 'n eom ordinary el all their" through th 4, uniting thelw 7I 'repr'esen .neetingihe retort i1 2, fen" zari ends 'of exazizftly hefurnace mrtion;

is composed eft a "i; hating nt, each shelled The'pe :3

at both ends, ut having inwerdly. to embrace the orlees sffiabmcefionamma Patent 7 3'9 ieest Eerie No.,499,,2o2,.

Patented May 10, 1910'.

'4,fthe ends of which are secured Lions-1n the plate 8, secured to opand bottom the retort is provided: with 'cu- '1 -ved :doors 9, hingedthereto, and with twolpip-e's 10, each provided with aj eojek, such as11, 'scre'wed into'the eover. Eeeh of the d'o'orsis mounted on a rod 12,iii "l$ l3, projecting from' the body of the alt mm retort are mountedswing- I 14, adaptedtos wing down behind tions "15 on the cover,.thusfirmly locke c-ove'rsfl in position. Any desired eweirer, maybe adoptedfor fastenyers'to the retort. The top and ers arefpreeisely similar.ayer oi asbestos; or simiplaeed over the outer d'n the covers, andnetting 115 .the site-the co er por- Ods 12 by having pped around it, as

so the .eenter, and us run shafts 17,

. b he rods 17 When-it is desi move retort; theglpwerhalfo n' isremfived' i To ol the! p as ,A,:--,.B bound toget s'e th movedQI ro deWe St0 tending brackets a l offlie outside of thef ets arefirmly'fasteI-i. pitta-3 by be bolted'thereto, er made-integraltherewith, and have-f theirupper: parts-bent nut-- Wardly foreiigag'ementiwlth the-'ileteheshereinaftermentioned. With each of thebraek; ets 22 a pivoted latch lis' adhpted to'enga r ge two of these latchee being jpi-votally mounted on the part B, and two on the part C;Each latelr23 hes-it's end thickened, "as shown at 24, to own aroundthe. oer-responding basket 22, so that when .thehitches .are=in 1. m,termina ing arts A, B

-.o the parts B and O are p I 5; ,injthejus'ualmanner, which'areadaptedto on tracks 26,, so thetfihywh we co sisting of the we posltioli show i01}virhereby when the latchesflflei'ethrown up, the parts B andizG maybeseparated thereof. I 5% o we rddutsbf passe thro. h h

from theretort whex'geupoli .the letter may bfi roteiged-lh meaneof powapp ed toitl e ded with a latsih 29;

e form of serve to the; ohimn thickened, '.as' I shjcw at 32;; igm'idthickened end haying a groove' the in iior the d bf the. retort"-which-i; eopeh endof-the pm isle apted retortA;lea ingth1etter','ejtorotete,

The ifdplatibn is; as f'oflowsb The appa rati s; be ng in thepositionfshownj in Fig'. 1;

if itis deslred-to nieke gas, .cbk'eg end ag geto teleseo e.I'; Thiserrengemenfli's. edapted so that t e parts Bggnd L G may be ,mov'ed g te t ee Qu fb mg f m a w h ee torfiarbon, for" example, the upper door Iof the retort is .opened,ia.nd va' suitable" charge obsofl;eoalvintroduced into theint'ei'ior 01E 7':

' fsai'dretort ilito-jthe space between the pipes andoonneetlonsmadeibetwe en the ,'scharg'e pipes lq efiythe top oftheretort leading t'o,

'the ge'soh -eter, or tofiany place whereiga sfi-is 111 the retort A,the gases passing pumhrou h thediigcharge pipes 10 After. this opermtionha's-beencontinued fofaefiffieienttime,

ere diseng ez'fed from thebracktsQQ, andhe of e fltact-Wibh theretort A.All th'jeocks {we idieeon ectedo .flie pipes di gto 5 disconnectedrfrom'f the'rgab 4- both the. uppeifindilp opened. By means go.jron'mdg, tweenthe 111-116 7 is-iol eed-downgfqe soft coal and heat theSam lop-and bottom doofr's' to be useij- Afilf'is then. startedinthefurii Ina ce B; and-,the hot productfs offc'ombustion pass throughtheotubes 7 distilling the coal thb plie fIhe parts and Cferethenhrbughtback-131i; qo nnection-w ith v theglfetorp epdv 1110M down into,theiposltion e then connected .to-thef gas den e h ksr her The distihition process isih' v its close, and at hhe'end' th 11 Y a lowe do r vng' h pipes. 77, tithe wholefinterior oi-"the ret rt- 'fww laxer f e e eb F e sfactythatifthe Lew'renvlayer-o tain this-.beirbijn, -1 ch or anydesired kind of f iel' in bhe f" ma A5 theretort A becomes heatedup thegases from. the fqel pass outof -the upper' pip 10in the,usualfman'n'er, Ho en,-which 1, 9 1' 1'1 d vto run -ai'llo'th futureconsumptio A-descr'ib i niihe eserip tioh of th ap e o ks n collected.and

gafioinet er; and by means, f POW?r up 't-Qf-the pulle 18, theretort' isrotated pa.'reti1s,- th'e 'i'etoxtgi's-"revolved one 01; .more' timesduring-"the dis ti11 ation' process; .1

so that the dep'ositrof gas carbon withinthe retortI-fion the' filbes andwallsjthereofimay be: substantially-uniform j'There is left theretort;eokev and-wile sit-of .gas carbon.

Th former may be 13m ired by opening. the

:carbonon the tubes and on the inside of 3 the z q f fid pushing out thecoke from between the horif 1 zontel flu'es 7, leaving the deposit":ofg'zi' 1 This retort maybe then used when) it stands" or conveyed awa toanother portion of-'the' the three parts A,' B and r easing-the hearingground plant. by lal tchiil together and 1-5 the rodsor Shafts f 17.5

process is v frimerily designedt'ohtreet (31L Q in the clay, I mix withone part of clay six same;

- treatment of these clays) consist of the following partschemically"combined ri o esio en ogrr o 5 that isto say, one molecule of(ma-f alumina, two molecules of silica, two molecules of water, and-1 to3' per cent. of ferrous or ferricoxids or both, approximately stated.After determining the amount of alumina I tiines the amount of.lei-sulfate of sodium, as

compared with the alumina in the clay, basing the weights used upon theatomlc weights of the alumina and the bi-sulfate- .015 sodium; so thatthe latter salt may fur- "nish enough sulfuric acid to give up 3 mole-Qcules'of'said acid to the .alumina'.' In place I of clay, I may, ofcourse, use other ores of alumina, such as bauxite or coruhdu-mw The doquantity of bi-sulfate of sodium used should,

a k or course -be sufficient to furnish whatever iron ispresent w1th asufiiclent amount, of sulfur cjacid, as well as the alumma, baseduponthermolecular weights of the o'iiids of 5 iron and he-bii-sultate ofsodium. This mixture i hen heated in one .of 'myaretorts-producing adouble sulfate of aluminum and sodium represented by the formula -.Al(SO ,3Na SO ierric alum sulfate of soda, and free silica, according. tothe follow- 7 ing reaction n shone :be mentio'ned that the retort shouldonlyfl be charged so that it isfabout tort-it isseparated from the"furnace B and fchimney connecting -portion- C and revolved,

T thus thoroughly 1 inixi'ng' ;-th'e materials jtogetheri" Thenftheth'ree"parts AQJfB and C are reunited, as shown inFig. 1 and-there; tortis'heated by the =f1' 1rnace B. Sulfuric acid is set free fromfthebi andattacks the} Gay; mass 1;be'come s f of a a; dark/ blue color and" boilsrapidlyg an there: is a rapid ein-unmet steam, Ferric alum is'formediand alsoa new compound consisting of a double sulfate ofaluminum and sodium, but haVingIB' molecules of sul-v fate ofsodacombined with '1- molecule of sulfate of aluminum. During the samereaction sillca 1s also formed 1n an anhydrous condition, and when thereaction is.ended,' the mass assumes-a dirty yellow-ishwhite "thefOllOwl atmNa FAL-ea sulfate 0fsodium 1 dens'ed' in the usual The upperand lower.

the contents of the retort. Thefdoublei sul f fates aredissolved outof'the'fused'm-asg. c

leaving the silica in an insoluble forms" The mass of material obtainedbyw -ashi ng out. I

the retorts is tllGI-L filtered, sepamtingthe silica, which is washedagain, if necessit and is then in a fine -whiteconditioralai f.-

mirably suited formaking glass and other;

purposes for which silica is'co'minenly used.

If clay is fused with acidrscdium sulfate,

NaHSO the iron in solution is precipitated with sodium prussiate. -Theprecipitated ferric prussiat-e is treated withcaustic soda,

and the prussiate of sodium recovered to be used over and overagain.

It will be noted that by myprocess the sulfate of alumina is unitedchemically with 3 molecule-sot sulfate of soda instead of with 1molecule, as in ordinary-alum, and by making use of'thi 'newdouble-sulfate, I have/devised an improved soda process.- This doublesulfat fusedinone-of my retorts with cry'ol' i muse ent in the re'torofaluminum -isproduced,- which is-"insoluble?" Sulfate of soda is alsopro-- duced, which is allowed to partially cool and while stillihot' islixiviated and the fluorid of "aluminum;separated from the solution ofthe sulfate of soda by filtration. The fiuorid' is; soluble;

offalilminum, after'being allowed to dry,

is heated to about "redness and showered down upon melted metallicsodium, whereupon-the following reaction takes place:

This reaction results-in the production of metallic 'aluininuin andcryolite. At the- 1 sameti-me a slag is formed which maybe au'sed tofuse with the product obtained from claysaftr'iiusingthem withbi-siilfat-e of idium, as mentioned, above.

portions'indicated by" T carbon being p-resr The mixture I obtain"metallic 'sbdium as follows": The sulfate of soda already obtainedisaplac'ed in oneofthe retorts 'A,; tvhich"hasbeen-lined w t f m a Pr vou y d s ri e Qoke',;iinely pulverized; niayf-thenbe a'd de'd, 1fnecessary, and the retort is then heated,

whereupon sulfidof soda is produced, there i :still being an excess 'ofcarbon left in there tort. Caustic lime is then added and there-'tortheated to about 800 (3., when-metallic sodium commences to distiloverand-is conmanner, the reaction be",

ing as follows: p GNafi-l-GCaO-l-6C:6Na +6CaS-{-6CQ:. In other words, Iproduce inetallic sodium indirectly from the sulfate of sodium or di-'rectly from the sulfid. I .use' lime to take the sulfur from the sodium,forming sodium, oxid,'which is immediately reduced tdmetallic sodium bythe carbon present in the retort. I also manufacture aluminate of soda,

Al O 3Na O, in a, similar manner; that is,

I place the double sulfate of soda and alumina already obtained in oneof my carbon lined retorts, and heat it until the sulfate of alumina isdecomposed, forming the "oxid. Sulfurous acid gas is driven ofi,-passesover carbon monoxidand dioxid into a discharge pipe, which leads into asulfuric acid chamher, where the, usual treatment for making sulfuricacid takes place. There is left in the retort alumina either mixed orchemically combiner! with 3 moleculesof sulfid of sodium, Al,O 3Na' S. Ithen add caustic lime in suflicient quantities to take up the sulfur,whereupon the following reaction.

' "I The aluminate of soda thus produced is nate of sodathroun'ha leadpipe. The .following reaction'takes place: al o sn oiiain y vThehydrofluoric" acid is rapidly condensed andartifieial cryolite isprecipitated. Carbonate of soda may also be produced as follows:,Carbonate of lime is heated in oneof my retorts and the carbonic acidpro- "dueed is led away and stored up for use.

- 'Aluminate of soda in solution is then treated with this. gas,whereupon the hydrate of aluminais precipitated, while carbonate of sodaIBIIIELHIS in solution, *Whenever icarbonates orcaustic alkalies areheated at a red heat, the difiiculty has been to keep the carbon, whichis lighter than the material treated, always in contact with the entiremass of the melted materiaL;

In my retort, the gas. carbon. is fixed around the time andonter ortion'of the retort and held thereimlnova .ly,'-ac cording of alumina soda,ferric alum, and free silica may bmproduced, as well as .fluomd to thereactions already set, forth. According to my method, a new doublesulfate of aluminium, sulfate of soda, metallic alumi The mass isallowed to cool and treat:

aluminate of soda, besides various others.

7 num, artificial cryolite, metallic sodium,

"Ina complete plant I design" to useone series or battery of my retortswithout distilling coal in them at all, and in another series, where' it1s desirable to use a carbon lined retort, coal 1s d1st1lled, forminggas and a fresh lining of graphite or fresh carbon at every.dlstillation, taking care in every distillin operation to tip the retortover, so that t e "bottom door is on the top and vice versa. The retort,is preferably suspended from above by hangingsupports, the bottom half;bearings being lifted up to the shaft by bolts and screws, as shown inthe-drawing. The retort is detachably fixed' to the furnace and chimneconnecting portions by .means of cylin fitting into circular grooves,and these-with the. latches support the retort A when it is releasedfromits bearings, so that the whole structure; consisting ,ofthe three partsA, B and G'may berolled away to "another part of the plant.

ing' ores containing alumina, silica and iron,

theste which consists in heating them in. a close retort wlth an excessof bi-sulfate of soda, producing thereby a double sulfate of alumina andsoda, containing three molecules of sulfate of soda'to one molecule ofsulfateof alumina, a ferric alum and free silica, substantially asdescribed.

' 2. In the herein described process, the step 1. In the hereindescribed processof treatrical proj ections which consists inheatingclays in. a closed retort with, an excess of bi-sulfate of soda,

producing a double sulfate of soda andalumina, having three molecules ofsulfate of soda to one molecule of sulfate of alumina,andjfree silica,and separating said double sulfate from said silica, substantially asdescribed. i v

3.' The herein described process of making aluminum fluorid, whichconsists in heating clay in a closed retort with an excessof bisulfateof soda, forming a double sulfate of alumina and soda, having threemolecules of sulfateof soda to one molecule of sulfate of alumina,separating out *said double sulfate, ,7

' heating it in a carbbndined retort, heating g the resulting productwith lime, dissolving out aluminate of soda from the product and leadinginto'the solution thus formed a stream of" hydrofluoric acid gas,-substantially as"described. w

In testimony whereof, I aflix my signa ture, in presence offiwowitnesses.

' rHILIP A. EMANUEL. Witnesses: 7 I S. SonosKr,

